CN1887923A - Prepn of low molecular weight polyacrylamide - Google Patents
Prepn of low molecular weight polyacrylamide Download PDFInfo
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- CN1887923A CN1887923A CN 200610048457 CN200610048457A CN1887923A CN 1887923 A CN1887923 A CN 1887923A CN 200610048457 CN200610048457 CN 200610048457 CN 200610048457 A CN200610048457 A CN 200610048457A CN 1887923 A CN1887923 A CN 1887923A
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Abstract
The present invention discloses preparation process of low molecular weight polyacrylamide, and the preparation process is one water solution polymerization process with ethanol as heat transferring solvent, sodium formate as chain transferring agent, ammonium persulfate as initiator, and EDTA disodium salt as stabilizer. Through continuously dropping of acrylamide solution and initiator solution, reflux polymerization at 80-90 deg.c and regulating the consumption of sodium formate and initiator, polyacrylamide of molecular weight (1.0-2.6)*10<4> is synthesized. Thus synthesized low molecular weight polyacrylamide has excellent water solubility, and is suitable for use as polymer emulsifier, dispersant, adhesive, etc.
Description
Technical field
The present invention relates to the synthetic method of macromolecular compound polyacrylamide, relate in particular to a kind of synthetic method of low molecular weight polyacrylamide.
Background technology
Lower molecular weight (molecular weight＜20 * 10
4) polyacrylamide is applied to fields such as building decoration, papermaking, weaving, printing and dyeing, pottery, jointing material, chemical industry as tackiness agent, additive.Because the polymerization activity height of acrylamide monomer, reaction heat is big, and the synthetic preparation in industrial production and laboratory low molecular weight polyacrylamide is difficulty relatively.Domestic have document announcement to adopt the synthetic low molecular weight polyacrylamide of precipitation polymerization method, but synthesis step is loaded down with trivial details, complex process, and use a large amount of organic solvents, be unfavorable for safety in production.It is comparatively feasible to adopt aqueous solution polymerization method to synthesize on the low molecular weight polyacrylamide technology, is 20% o'clock as Ningbo chemical research institute in monomer mass concentration, is initiator system with the ammonium persulfate-sodium bisulfite, synthesizes molecular weight and is (23～40) * 10
4Polyacrylamide; It is 10% o'clock that Nantong Vocational College's chemical engineering ties up to monomer mass concentration, is initiator system with Potassium Persulphate-nitrogen tripropyl amine, and synthesizing molecular weight is 62 * 10
4Polyacrylamide.In sum, the water solution polymerization process prior art generally adopts the synthetic low molecular weight polyacrylamide of 10%～20% low monomer concentration, and its molecular weight ranges is generally in (23～62) * 10
4Between.
The main inventor of present technique in ZL03126303.8, was chain-transfer agent and heat transferring solvent with the Virahol once, was 30% o'clock in monomer mass concentration, synthesized molecular weight＜20 * 10
4Polyacrylamide, minimum is 2.6 * 10
4, but being difficult to synthetic more low-molecular-weight polyacrylamide, monomer concentration can not further improve, and has the low and higher problem of cost of production efficiency.For this reason, the present invention is further improved on this basis.
Summary of the invention
The object of the present invention is to provide a kind ofly under high monomer concentration, adopt aqueous solution polymerization to synthesize molecular weight ranges in (1～2.6) * 10
4The method of low molecular weight polyacrylamide, make the low molecular weight polyacrylamide that synthesizes water-soluble good, production cost reduces.
In order to realize goal of the invention, technical solution of the present invention is as follows: adopting water solution polymerization process, is heat transferring solvent with ethanol, sodium formiate is a chain-transfer agent, ammonium persulphate is an initiator, and disodium EDTA (EDTA) is a stablizer, synthesizes low molecular weight polyacrylamide by following steps:
(1) acrylamide solution and the 5～25g sodium formiate mixed dissolution with 200g mass percent concentration 40% is made into monomer solution, and 0.5～1.2g ammonium persulphate is dissolved in the 10g water and is made into initiator solution.
(2) in flask, add 50g95% ethanol, the above-mentioned monomer solution for preparing of 20g, the 2g mass concentration is 3% EDTA solution, 1.2g the above-mentioned ammonium persulfate initiator solution for preparing, start stirring, progressively be warming up to 80 ℃ of backflows, kept reflux temperature 10 minutes.
(3) keeping under stirring and the reflux state, from constant pressure funnel, dripping residual monomers solution and remaining initiator solution respectively continuously, in 2 hours, dropwising.
(4) backflow keeps reaction 2 hours, under the atmospheric pressure state, steams ethanol and water mixture, and cooling obtains the low molecular weight polyacrylamide aqueous solution.
Measure the low molecular weight polyacrylamide that synthesizes according to GB17514-1998, its molecular weight is (1～2.6) * 10
4
Beneficial effect of the present invention is: this synthetic method adopts aqueous solution polymerization, has simplified polymerization technique, has improved monomer concentration, and the synthetic Molecular Weight for Polyacrylamide is lower, control easily, operational safety and reduced production cost.Method synthetic low molecular weight polyacrylamide has good water-solubility thus, is applicable to make macromolecule emulsifier, tackiness agent etc.
Embodiment
For the present invention will be described better, it is as follows to enumerate embodiment:
Embodiment 1
(1) be that 40% acrylamide solution and 5g sodium formiate mixed dissolution are made into monomer solution with the 200g mass percent concentration, the 0.6g ammonium persulphate is dissolved in the 10g water and is made into initiator solution.
(2) at 0.5L adding 50g95% ethanol in electronic stirring, constant pressure funnel, thermometer, the reflux exchanger four-hole boiling flask is housed, the above-mentioned monomer solution for preparing of 20g, the 2g mass concentration is 3% EDTA solution, 1.2g the above-mentioned ammonium persulfate initiator solution for preparing, start stirring, progressively be warming up to 80 ℃ of backflows, kept reflux temperature 10 minutes.
(3) keeping under stirring and the reflux state, from constant pressure funnel, dripping residual monomers solution and remaining initiator solution respectively continuously, in 2 hours, dropwising.
(4) backflow keeps reaction 2 hours, under the atmospheric pressure state, steams ethanol and water mixture, and cooling obtains the low molecular weight polyacrylamide aqueous solution.
Measuring its molecular weight by GB17514-1998 is 2.28 * 10
4
Embodiment 2
With embodiment 1, changing the sodium formiate consumption is 8g, and the low molecular weight polyacrylamide solution that is obtained is 2.07 * 10 by the GB17514-1998 determining molecular weight
4
Embodiment 3
With embodiment 1, changing the sodium formiate consumption is 15g, and resulting low molecular weight polyacrylamide is 1.47 * 10 by the GB17514-1998 determining molecular weight
4
Embodiment 4
With embodiment 1, changing the sodium formiate consumption is 17.5g, and resulting low molecular weight polyacrylamide solution is 1.0 * 10 by the GB17514-1998 determining molecular weight
4
Embodiment 5
(1) be that 40% acrylamide solution and 5g sodium formiate mixed dissolution are made into monomer solution with the 200g mass percent concentration, the 0.8g ammonium persulphate is dissolved in the 10g water and is made into initiator solution.
(2) implementation step is with (2) (3) (4) (5) among the embodiment 1.
It is 1.55 * 10 that resulting low molecular weight polyacrylamide solution is measured its molecular weight by GB17514-1998
4
Embodiment 6
With embodiment 5, the change ammonium persulphate is 1.2g, obtains low molecular weight polyacrylamide solution, and measuring its molecular weight by GB17514-1998 is 1.81 * 10
4
The low molecular weight polyacrylamide solution that this method synthesizes has good water-solubility, is applicable to macromolecule emulsifier, dispersion agent, tackiness agent etc., has market outlook preferably.
Claims (2)
1, a kind of preparation method of low molecular weight polyacrylamide, adopt water solution polymerization process, it is characterized in that: selecting ethanol for use is heat transferring solvent, sodium formiate is a chain-transfer agent, ammonium persulphate is an initiator, disodium EDTA is a stablizer, and by the synthetic low molecular weight polyacrylamide of the consumption of regulating chain-transfer agent sodium formiate and initiator ammonium persulfate, concrete steps are as follows:
(1) be that 40% acrylamide solution and 5～25g sodium formiate mixed dissolution are made into monomer solution with the 200g mass percent concentration, 0.5～1.2g ammonium persulphate is dissolved in the 10g water and is made into initiator solution;
(2) adding 50g95% ethanol, the above-mentioned monomer solution for preparing of 20g, 2g mass percent concentration in flask is 3% the above-mentioned ammonium persulfate initiator solution for preparing of disodium EDTA solution, 1.2g, stir, progressively be warming up to 80 ℃ of backflows, kept reflux temperature 10 minutes;
(3) keeping under stirring and the reflux state, from constant pressure funnel, dripping residual monomers solution and remaining initiator solution respectively continuously, in 2 hours, dropwising;
(4) backflow keeps reaction 2 hours, steams ethanol and water mixture under the atmospheric pressure state, and cooling obtains the low molecular weight polyacrylamide aqueous solution.
2, preparation method as claimed in claim 1 is characterized in that, the prepared low molecular weight polyacrylamide molecular weight that goes out is 1 * 10
4～2.6 * 10
4
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100484575A CN100384891C (en) | 2006-07-26 | 2006-07-26 | Prepn of low molecular weight polyacrylamide |
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| CNB2006100484575A CN100384891C (en) | 2006-07-26 | 2006-07-26 | Prepn of low molecular weight polyacrylamide |
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| CN1887923A true CN1887923A (en) | 2007-01-03 |
| CN100384891C CN100384891C (en) | 2008-04-30 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054575B (en) * | 2007-04-03 | 2011-07-27 | 沈阳化工学院 | Preparation method for modified polyacrylamide immobilization cell |
| CN102391404A (en) * | 2011-08-30 | 2012-03-28 | 河南省科学院高新技术研究中心 | Method for preparing low molecular weight polyacrylamide with molecular weight of 100,000 to 250,000 |
| CN102432721A (en) * | 2011-09-14 | 2012-05-02 | 河南省科学院高新技术研究中心 | Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 |
| CN102690381A (en) * | 2012-06-21 | 2012-09-26 | 河南省科学院高新技术研究中心 | Preparation method of ultralow-molecular-weight (5000-20000) polyacrylamide |
| CN103435727A (en) * | 2013-09-06 | 2013-12-11 | 河南省科学院高新技术研究中心 | Preparation method of low molecular weight (LMW) polyacrylamide with molecular weight of 0.4-1 million |
| CN105111342A (en) * | 2015-09-18 | 2015-12-02 | 河南省科学院高新技术研究中心 | High-concentration acrylamide water solution polymerization method |
| CN105111343A (en) * | 2015-09-23 | 2015-12-02 | 山东聚鑫化工有限公司 | Preparation method of salt-resistant low molecular weight polyacrylamide |
| CN114163555A (en) * | 2021-12-29 | 2022-03-11 | 扬州科苑化工有限公司 | Polyacrylamide dispersant and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5932671A (en) * | 1997-06-04 | 1999-08-03 | Phillips Petroleum Company | Polymerization process |
| CN1232548C (en) * | 2003-08-12 | 2005-12-21 | 河南省科学院质量检验与分析测试研究中心 | Method for preparing low molecular weight polyacrylamide |
-
2006
- 2006-07-26 CN CNB2006100484575A patent/CN100384891C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054575B (en) * | 2007-04-03 | 2011-07-27 | 沈阳化工学院 | Preparation method for modified polyacrylamide immobilization cell |
| CN102391404A (en) * | 2011-08-30 | 2012-03-28 | 河南省科学院高新技术研究中心 | Method for preparing low molecular weight polyacrylamide with molecular weight of 100,000 to 250,000 |
| CN102432721A (en) * | 2011-09-14 | 2012-05-02 | 河南省科学院高新技术研究中心 | Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 |
| CN102432721B (en) * | 2011-09-14 | 2013-07-31 | 河南省科学院高新技术研究中心 | Method for synthesizing polyacrylamide having low-molecular weight of 200000 to 450000 |
| CN102690381A (en) * | 2012-06-21 | 2012-09-26 | 河南省科学院高新技术研究中心 | Preparation method of ultralow-molecular-weight (5000-20000) polyacrylamide |
| CN103435727A (en) * | 2013-09-06 | 2013-12-11 | 河南省科学院高新技术研究中心 | Preparation method of low molecular weight (LMW) polyacrylamide with molecular weight of 0.4-1 million |
| CN103435727B (en) * | 2013-09-06 | 2015-07-01 | 河南省科学院高新技术研究中心 | Preparation method of low molecular weight (LMW) polyacrylamide with molecular weight of 0.4-1 million |
| CN105111342A (en) * | 2015-09-18 | 2015-12-02 | 河南省科学院高新技术研究中心 | High-concentration acrylamide water solution polymerization method |
| CN105111342B (en) * | 2015-09-18 | 2017-04-05 | 河南省科学院高新技术研究中心 | A kind of high concentration polymerization of aqueous solution of acrylamide method |
| CN105111343A (en) * | 2015-09-23 | 2015-12-02 | 山东聚鑫化工有限公司 | Preparation method of salt-resistant low molecular weight polyacrylamide |
| CN114163555A (en) * | 2021-12-29 | 2022-03-11 | 扬州科苑化工有限公司 | Polyacrylamide dispersant and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100384891C (en) | 2008-04-30 |
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Assignee: Zhengzhou Zhengli Polymer Technology Co., Ltd. Assignor: Quality Check and Analysis Test-Reseach Center, Henan Prov. Academy of Sciences Contract fulfillment period: 2009.4.17 to 2019.4.16 contract change Contract record no.: 2009410000064 Denomination of invention: Prepn of low molecular weight polyacrylamide Granted publication date: 20080430 License type: Exclusive license Record date: 2009.4.22 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.17 TO 2019.4.16; CHANGE OF CONTRACT Name of requester: ZHENG ZHOU ZHENGLI POLYMER SCIENCE CO., LTD. Effective date: 20090422 |
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